WO2012132007A1 - Process and apparatus for producing regenerated tobacco material - Google Patents

Process and apparatus for producing regenerated tobacco material Download PDF

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Publication number
WO2012132007A1
WO2012132007A1 PCT/JP2011/058341 JP2011058341W WO2012132007A1 WO 2012132007 A1 WO2012132007 A1 WO 2012132007A1 JP 2011058341 W JP2011058341 W JP 2011058341W WO 2012132007 A1 WO2012132007 A1 WO 2012132007A1
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WIPO (PCT)
Prior art keywords
membrane
fractionation
tobacco extract
tobacco
microbubbles
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PCT/JP2011/058341
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French (fr)
Japanese (ja)
Inventor
毅 二村
阿部　進
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日本たばこ産業株式会社
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Priority to PCT/JP2011/058341 priority Critical patent/WO2012132007A1/en
Publication of WO2012132007A1 publication Critical patent/WO2012132007A1/en

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    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B3/00—Preparing tobacco in the factory
    • A24B3/14—Forming reconstituted tobacco products, e.g. wrapper materials, sheets, imitation leaves, rods, cakes; Forms of such products
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18—Treatment of tobacco products or tobacco substitutes
    • A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts

Definitions

  • the present invention relates to a method for producing a recycled tobacco material and an apparatus used for the method.
  • Tobacco materials such as natural tobacco leaves, chops, bones, stems and roots contain various components such as nicotine, nitrates, nitrosamines, hydrocarbons and proteins. Extracting these components from natural tobacco materials and using them as a taste additive for tobacco has been carried out. In that case, there is a component that is desired to be reduced or removed (undesirable component) for taste or for other reasons, while another component (desired component) that is desired not to be removed or increased in concentration is also desired. is there. Desired components include amino acids, sugars, nicotine, foliar resins, alkaloids, and undesired components include nitrates and nitrosamines such as tobacco specific nitrosamine (TSNA).
  • TSNA tobacco specific nitrosamine
  • Patent Document 1 extracts a natural tobacco material, obtains a tobacco extract and an extraction residue, and converts the tobacco extract into a membrane using an ultrafiltration membrane or a reverse osmosis filtration membrane (collectively referred to as a fractionation membrane).
  • a first fraction enriched with desired components and subjected to fractionation and subjected to fractionation, and a second fraction enriched with unwanted components and enriched with unwanted components A method for producing a recycled tobacco material is disclosed.
  • a recycled tobacco web is prepared using the extraction residue, and a recycled tobacco material is produced by adding the first fraction to the web.
  • Patent Document 2 discloses a treatment liquid containing microbubbles such as microbubbles and nanobubbles (substances attached to a fractionation membrane are brought into contact with the fractionated membrane by bringing filtered water from the fractionation membrane or raw water supplied to the fractionation membrane into contact with the fractionation membrane. Is disclosed.
  • tobacco extract contains a relatively large amount of sugar and protein, and when it is subjected to fractionation using a fractionation membrane, washing with a treatment liquid containing microbubbles and nanobubbles can sufficiently remove the adhered substances. Absent.
  • the present invention enables continuous and efficient separation of desired and undesired components in tobacco extract by a fractionation membrane (ultrafiltration membrane or reverse osmosis membrane). It is an object to provide a method for producing a regenerated tobacco material that contains components but has a significantly reduced amount of undesired components.
  • the present invention provides a fractionation membrane for continuously and efficiently obtaining a fraction containing a significant amount of a desired component but a significant amount of an undesirable component removed from a tobacco extract.
  • An object of the present invention is to provide a device.
  • a natural tobacco material is extracted with an extraction solvent to obtain a tobacco extract containing the desired and undesired components and an extraction residue, and (b) the tobacco extract.
  • C removing precipitates deposited in the tobacco extract by contact with the microbubbles;
  • D ultrafiltration of the tobacco extract from which the deposits have been removed.
  • a first fraction containing the desired component and having the undesired component deteriorated by being subjected to a fractionation operation using a membrane or a reverse osmosis membrane;
  • preparing a regenerated tobacco web containing the extraction residue and (f) adding the first fraction to the regenerated tobacco web.
  • a fractionation device for separating a desired component and an undesired component in a tobacco extract, a first container containing a tobacco extract, and generation of microbubbles
  • An apparatus and a first feeding device for feeding the generated microbubbles to the first container for treating the tobacco extract with the microbubbles to deposit precipitates from the tobacco extract (E.g., a pump), a tobacco extract treated with the microbubbles, a first fraction containing the desired component and the undesired component is degraded, and the desired component is degraded.
  • a fractionation device comprising an ultrafiltration membrane or a reverse osmosis membrane that fractionates into a second fraction enriched in the undesired components.
  • the present invention allows continuous and efficient separation of desired and undesired components in tobacco extract by ultrafiltration membranes or reverse osmosis membranes, thus containing significant amounts of desired components but not Recycled tobacco materials with significantly reduced desired components can be produced.
  • FIG. 1 is a schematic diagram of a fractionation apparatus according to one embodiment of the present invention.
  • FIG. 2 is a diagram showing the results of Example 1, which will be described in detail later, together with the results of a comparative example.
  • FIG. 3 is a diagram showing the results of Example 1 described in detail below together with the results of Comparative Examples.
  • One aspect of the present invention relates to a method for producing a regenerated tobacco material using a tobacco extract obtained by extracting a natural tobacco material and an extraction residue.
  • the regenerated tobacco web containing the extraction residue is manufactured.
  • the tobacco extract is brought into contact with the microbubbles, and deposits deposited in the tobacco extract as a result of the contact are removed.
  • the tobacco extract from which the precipitate has been removed is subjected to a fractionation operation using a fractionation membrane (ultrafiltration membrane or reverse osmosis membrane). By this fractionation operation, a first fraction containing a desired component and an unwanted component is poored, and a second fraction in which the desired component is poored and the unwanted component is enriched can get.
  • the desired regenerated tobacco material is produced by adding the first fraction to the regenerated tobacco web.
  • the natural tobacco material and the extraction solvent are mixed and stirred.
  • the natural tobacco material tobacco leaf, its chop, middle bone, stem, root and a mixture thereof can be used.
  • the extraction solvent water or a mixture of water and a water-miscible organic solvent can be used.
  • water-miscible organic solvents are alcohols such as ethanol, ethers such as diethyl ether, and the like.
  • the extraction treatment can usually be performed at a temperature of 0 to 100 ° C. for 5 minutes to 6 hours.
  • the obtained extraction mixture is subjected to a separation operation such as filtration, centrifugation, etc., and separated into tobacco extract and extraction residue.
  • Natural tobacco materials include metal salts such as potassium, nitrates, nicotine, sugars such as sucrose, amino acids, glycosides, amino-sugar compounds, proteins, hydrocarbons (saturated hydrocarbons, unsaturated carbonization) Hydrogen, aromatic hydrocarbons), alcohols, ethers, aldehydes, ketones, esters, lactones, quinones, acids (including acid anhydrides), phenols, amines, pyrroles, pyridine , So-called pyrazines, alkaloids, polycyclic nitrogen-containing compounds, nitroso compounds such as nitrosamines (including TSNA), amides, lipids, halides, sulfur-containing compounds, inorganic elements and the like.
  • metal salts such as potassium, nitrates, nicotine, sugars such as sucrose, amino acids, glycosides, amino-sugar compounds, proteins, hydrocarbons (saturated hydrocarbons, unsaturated carbonization) Hydrogen, aromatic hydrocarbons), alcohols,
  • the tobacco extract obtained by the extraction treatment can contain most of these components, although depending on the type of extraction solvent used.
  • desired components include amino acids, sugars, nicotine, foliar resin, and alkaloids
  • undesired components include nitrosamines such as nitrates and TSNA.
  • TSNA nitrosamines (N′-nitrosonornicotine (NNN), 4- (methylnitrosoamino) -1- (3-pyridyl) -1-butanone (NNK), N′-nitrosoanatabine (NAT) N′-nitrosoanabasin (NAB).
  • the extraction residue is a component that is insoluble in the extraction solvent and substantially consists of fibers.
  • a regenerated tobacco web is produced by a conventional method.
  • a part of the regenerated tobacco web may be constituted by an extraction residue, or the whole may be constituted by an extraction residue.
  • a pulp material containing an extraction residue can be made into a recycled tobacco web by paper making in a normal paper making process.
  • the tobacco extract (hereinafter sometimes referred to as “stock solution”) is contained in a stock solution container and brought into contact with microbubbles generated by a microbubble generator.
  • stock solution contains a stock solution container and brought into contact with microbubbles generated by a microbubble generator.
  • Microbubble generation mechanisms and generators are well known in the art and will not be described here.
  • Microbubble generators are commercially available. Microbubbles can be generated using a stock solution, or can be generated using a membrane permeate or a membrane impermeate fractionated by a fractionation membrane described later.
  • the microbubbles can have a diameter of 0.000005 mm to 0.1 mm. Microbubbles can be introduced into a stock solution container and pretreatment with microbubbles can be performed.
  • the removal of the precipitate includes that the precipitate is separated from the stock solution as a result of the precipitate floating on the surface of the stock solution.
  • a batch of tobacco extract from which precipitates have been removed is stored in a pre-treated liquid container, sent from there to a fractionation membrane, and subjected to fractionation operation with a fractionation membrane to give a membrane permeate fraction and a membrane-free fraction. Fractionate into permeate fraction.
  • the membrane permeate fraction is enriched with undesirable components including TSNA.
  • the membrane impermeate fraction is poor in unwanted components including TSNA.
  • the membrane-impermeable fraction can substantially maintain the initial amount of desired component (eg nicotine) in the tobacco extract (85% by weight or more), correspondingly the membrane-permeate fraction Is substantially not included.
  • the reverse osmosis membrane allows the undesired component to permeate but does not substantially permeate the desired component.
  • the reverse osmosis membrane is preferably one that does not allow permeation of soluble components (excluding TSNA) such as sugar in the tobacco extract.
  • a reverse osmosis membrane having a pore diameter of 0.1 to 3 nm can be used.
  • the reverse osmosis membrane may be a flat membrane, a bag-shaped one formed into a cylindrical shape (spiral membrane), or a hollow fiber membrane or a tubular membrane.
  • the tobacco extract can be supplied to the reverse osmosis membrane at a pressure of 1 to 3 MPa.
  • the tobacco extract can be supplied to the reverse osmosis membrane using a high-pressure pump.
  • the membrane impermeate fraction is enriched with unwanted components, and the membrane permeate fraction is correspondingly enriched with unwanted components.
  • the range of the molecular weight cut off of the ultrafiltration membrane is 1,000 to 1,000,000.
  • the fraction in which the undesirable components are deteriorated can be returned to the pretreated liquid container and sent again to the fractionation membrane to perform the fractionation operation.
  • the amount of undesired components such as TSNA is, for example, about 40% by weight or less of the initial amount (TSNA removal rate of 60% by weight or more), or 20% by weight or less (TSNA removal rate of 80% by weight or more), Further, the process can be repeated until it is 10% by weight or less (TSNA removal rate is 90% by weight or more).
  • the desired component eg, nicotine
  • the same fractionation operation is performed on the next batch of tobacco extract. It is preferable that such a fractionation operation is continuously repeated for a plurality of batches of tobacco extract, then the fractionation operation is stopped and the fractionation membrane is washed.
  • This fractionation membrane can be washed using water containing microbubbles (cleaning solution) obtained by passing water through a microbubble generator. This cleaning liquid is accommodated in a pretreatment liquid container, and sent from there to the fractionation membrane to wash the fractionation membrane.
  • the membrane permeate and membrane impermeate of the cleaning liquid are returned to the pretreatment liquid container, the cleaning liquid is sent again to the microbubble generator, and the obtained processing liquid (cleaning liquid) containing the microbubbles is sent again to the pretreatment liquid storage container.
  • the treatment liquid (cleaning liquid) is sent from the pretreatment liquid storage container to the fractionation membrane and washed. After such a washing cycle is repeated for a predetermined time, the washing operation is stopped and the tobacco extract liquid fractionation operation is restarted.
  • ozone can be introduced into the cleaning liquid containing microbubbles.
  • Ozone can be generated from an ozone generator and introduced into a pretreatment liquid as a cleaning liquid from the pretreatment liquid storage device toward the fractionation membrane for cleaning. This ozone treatment further improves the cleaning efficiency of the fractionation film.
  • the separation membrane may be heated with warm water (temperature 40 to 100 ° C.) and / or an alkaline aqueous solution (for example, sodium hydroxide aqueous solution or sodium lauryl sulfate). It can also be washed with an aqueous solution of an alkaline surfactant.
  • warm water temperature 40 to 100 ° C.
  • alkaline aqueous solution for example, sodium hydroxide aqueous solution or sodium lauryl sulfate. It can also be washed with an aqueous solution of an alkaline surfactant.
  • FIG. 1 is a schematic diagram of a fractionation apparatus 10 according to one aspect of the present invention, and an aspect having a reverse osmosis membrane as a fractionation membrane will be described.
  • a fractionation device 10 shown in FIG. 1 includes a container 111 for storing an extract (stock solution) TEL obtained by the extraction process of the natural tobacco agent, a container 112 for storing a pretreated tobacco extract TTE by microbubbles, A microbubble generator 113 and a fractionation device 114 including a fractionation film 1141 are provided.
  • upstream and downstream are based on the liquid flow direction.
  • the bottom of the TEL container 111 communicates with the inlet of the pump P1 through a line L1 having an on-off valve V1, and the outlet of the pump P1 communicates with the inlet of the microbubble generator 113 through a line L2.
  • a line L3 including the on-off valve V2 communicates the outlet of the microbubble generator 113 and the top of the TEL container 111.
  • the bottom of the TEL container 111 communicates with the inlet of the pump P2 via a line L4 having an on-off valve V3, and the outlet of the pump P2 communicates with the top of the TTE container 112 via a line L5.
  • the bottom of the TTE container 112 communicates with the inlet of the pump P3 via a line L6 provided with the on-off valve V4, and the outlet of the pump P3 communicates with the inlet of the fractionation device 114 via the line L7 provided with the on-off valve V5. To do.
  • the membrane impermeate outlet of the fractionation device 114 communicates with the top of the TTE container 112 via a line L8 having an on-off valve V6.
  • the membrane permeate outlet of the fractionation device 114 is connected to a waste line L9 including an on-off valve V7.
  • the on-off valves V3, V4 and V5 are closed, the on-off valves V1 and V2 are opened, and the pump P1 is driven, whereby the stock solution (tobacco extract) in the TEL container 111 is supplied to the line L1 and the line.
  • L2 is introduced into the microbubble generator 113, microbubbles are generated by the microbubble generator 113, and the tobacco extract (pretreatment liquid) containing the microbubbles is transferred to the TEL container 111 via the line L3. Supply into the stock solution.
  • the separation membrane blocking substances such as saccharides, fats and proteins contained in the stock solution are precipitated from the stock solution and float on the surface of the stock solution.
  • the treatment of this floating substance was described above.
  • the on-off valve V1 is closed, the operation of the pump P1 is stopped, the on-off valve V3 is opened, and the pump P2 is driven, whereby one batch of pretreated stock solution in the container 111 (for example, 10 to 100 L), It introduces into the TTE container 112 via lines L4 and L5.
  • the on-off valve V3 is closed, the operation of the pump P2 is stopped, the on-off valves V4 to V7 are opened, and the pump P3 is driven, whereby the pretreated tobacco extract is transferred from the TTE container 112 to the fractionation device 114.
  • Supply sequentially In the fractionation device 114, the membrane impermeate fraction containing the desired component and the unwanted component such as TSNA being deteriorated by the fractionated membrane (reverse osmosis membrane in this embodiment) 1141. And a membrane permeate fraction enriched with undesired components such as TSNA.
  • the membrane-impermeable fraction is returned to the TTE vessel 112 via line L8, while the membrane-permeate fraction is discarded via line L9.
  • the amount of undesired components such as TSNA in the membrane-impermeable product fraction is, for example, about 40% by weight or less of the initial amount (TSNA removal rate of 60% by weight or more), or 20% by weight or less (TSNA).
  • the removal can be repeated until the removal rate is 80% by weight or more, and further 10% by weight or less (the TSNA removal rate is 90% by weight or more).
  • the desired component eg, nicotine
  • the membrane-impermeable fraction is successively concentrated by repeated fractionation operations.
  • the amount of undesired components in the membrane-impermeable material can be known, for example, by measuring the amount of TSNA in the discarded membrane-permeated fraction.
  • the concentrated tobacco extract contained in the TTE container 112 is recovered. Then, as described above, the next batch of pretreated tobacco extract is introduced from the TEL container 111 to the TTE container 112, and the same fractionation operation is performed.
  • the cigarette extract (stock solution) has been removed from the membrane occluding substance by pretreatment with a microvalve, so that compared to the case where such pretreatment is not performed, The decrease in permeation flux is suppressed to 50% or less, and the continuous fractionation processing time is significantly extended.
  • the fractionation device 10 includes a cleaning mechanism. More specifically, as shown in FIG. 1, the fractionation device 10 further includes a container 115 that stores the microbubble-containing liquid MBL.
  • a line L10 that communicates with the bottom of the MBL container 115 and has an on-off valve V8 is connected to the line L1 downstream of the on-off valve V1.
  • the bottom of the MBL container 115 communicates with the inlet of the pump P3 via a line L11 having an on-off valve V9.
  • a line L12 communicating with the outlet of the pump P3 is connected to the line L7 downstream of the on-off valve V5.
  • a line L13 that communicates with the top of the MBL container 115 and includes the on-off valve V10 is connected to the line L8 upstream of the on-off valve V6.
  • the line L14 includes the on-off valve V11.
  • a line L15 that communicates with the top of the MBL container 115 and includes an on-off valve V12 is connected to the line L3.
  • the fractionation device 10 preferably includes an ozone generator 116.
  • the ozone generator 116 is connected to the line L1 downstream of the on-off valve V1 via a line L16 provided with the on-off valve V13.
  • the non-membrane permeate fraction of the cleaning liquid is introduced into the MBL container 115 via lines L8 and L13, while the membrane permeate fraction of the cleaning liquid is also introduced into the MBL container 115 via lines L9 and L14.
  • the tobacco extract solution fractionation operation is restarted according to the above procedure.
  • the membrane in addition to washing the membrane with microbubbles, can be washed with warm water and / or an alkaline aqueous solution.
  • the fractionation device 10 shown in FIG. 1 includes a WW container 117 for containing hot water WW and / or an AL container 118 for containing an alkaline aqueous solution AL, as shown in FIG.
  • a line L17 that communicates with the bottom of the WW container 117 and includes the on-off valve V14 is connected to the line L6 downstream of the on-off valve V4.
  • a line L18 that communicates with the bottom of the AL container 118 and includes an on-off valve V15 is connected to the line L6 (via the line L17 in the example shown in FIG. 1).
  • a line 19 that communicates with the top of the WW container 117 and includes an on-off valve V16 branches off from the line L14 downstream of the on-off valve V11.
  • a line L20 that communicates with the top of the AL container 118 and includes the on-off valve V17 branches from the line L14 downstream of the on-off valve V11.
  • a line L21 that communicates with the top of the WW container 117 and includes the on-off valve V18 branches from the line L8 upstream of the on-off valve V6.
  • a line L22 that communicates with the top of the AL container 118 and includes the on-off valve V19 branches off from the line L8 upstream of the on-off valve V6.
  • the washing process of the fractionation membrane includes warm water washing and / or alkaline aqueous solution washing in addition to washing with microbubbles
  • the order of these two or three washing steps is not particularly limited. , Warm water cleaning, microphone bubble cleaning, and alkaline aqueous solution cleaning.
  • the cleaning process in that case will be described below with reference to FIG. 1 just in case.
  • the on-off valves V4, V5, V6 and V7 are closed, and the operation of the pump P3 is stopped.
  • the on-off valves V8, V9, V10, V12, V13, V15, V17, V19 are also closed, the on-off valves V14, V16, and V18 are opened, the pump P3 is driven, and the hot water WW is supplied from the WW container 117 to the lines L17, L6. And introduced into the fractionation device 114 via L7, and the fractionation film 1141 is washed.
  • the membrane permeate of warm water is returned to the WW container 117 via lines L8 and L21, while the membrane permeate of warm water is also returned to the WW container 117 via lines L14 and L19.
  • the on-off valves V16 and V18 are closed, and the membrane 1141 is washed with a cleaning solution containing microbubbles preferably containing ozone as described above.
  • the on-off valves V8 and V9 are closed, the on-off valves V15, V17 and V19 are opened, and the alkaline aqueous solution AL is introduced from the AL container 118 into the fractionation device 114 via the lines L18, L6 and L7.
  • the image film 1141 is washed.
  • the membrane-impermeable substance of the alkaline aqueous solution is returned to the AL container 118 via the lines L8 and L22, while the membrane-permeable substance of the alkaline aqueous solution is also returned to the AL container 118 via the lines L14 and L22.
  • the tobacco extract fractionation operation is restarted by the above-described method.
  • Example 1 and Comparative Example In this example, fractionation operation was performed using the apparatus shown in FIG.
  • As the reverse osmosis membrane Duratherm Excel RO 4040HR manufactured by GE Water Technologies was used.
  • TSNA total of NNN, NNK, NAT and NAB
  • the extracted residue was papered to obtain a regenerated tobacco web.
  • the tobacco extract was introduced into the TEL container 111.
  • microbubbles were generated by a microbubble generator 113 (Nagoya Oshima Co., Ltd.), a tobacco extract containing the microbubbles was introduced into the TEL container 111, and the deposited precipitates (floating matter) were removed.
  • the tobacco extract from which this precipitate has been removed is put into a batch (33.5 L) TTE vessel 112, and as described above, the membrane is continuously subjected to the fractionation operation by the fractionation membrane (reverse osmosis membrane) 1141. This was performed until the amount of TSNA in the impermeate fraction reached 4.5% of the initial amount (removal rate 95.5%).
  • the nicotine in the final membrane-impermeable fraction was maintained at about 86.6% of the initial amount.
  • the membrane impermeate fraction thus obtained was added to the regenerated tobacco web to obtain a reconstituted tobacco material.
  • 60 batches of tobacco extract were processed, and each time after 12 batches of tobacco extract were processed, the separation membrane was washed (washing with warm water at 78 ° C., washing with microbubbles and sodium hydroxide). Washing with an aqueous solution for each 20 minutes).
  • the fractionation operation was performed in the same manner as above except that the pretreatment of the tobacco extract with microbubbles was not performed.
  • FIG. 2 shows the ratio of membrane permeation flux (membrane permeation flux ratio) after treatment of one batch of tobacco extract to the initial membrane permeation flux in each case.
  • the membrane permeation flux was measured with a flow meter.
  • black circles indicate the results when pre-processing with microbubbles is performed, and x marks indicate the results when no pre-processing is performed.
  • Example 2 The same fractionation operation as in Example 1 was performed, and after each batch of tobacco extract was treated, the fractionation membrane was washed (washing with warm water at 78 ° C. and washing with aqueous sodium hydroxide solution for 20 minutes each). It was. In this way, the tobacco extract of 167 batches was fractionated and washed, and after the next 168th batch of tobacco extract was fractionated, washing with warm water at 78 ° C., washing with microbubbles and Washing with an aqueous sodium hydroxide solution was performed for 20 minutes each. At this time, ozone generated from an ozone generator 116 (manufactured by Nagoya Oshima Co., Ltd.) was supplied to the cleaning liquid containing microbubbles.
  • an ozone generator 116 manufactured by Nagoya Oshima Co., Ltd.

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Abstract

According to the present invention, a regenerated tobacco material is produced by: extracting a natural tobacco material with an extractant to obtain both a tobacco extract which contains desired components and undesired components and an extraction residue; bringing the tobacco extract into contact with microbubbles; removing the precipitate which has separated out in the tobacco extract, by the contact with the microbubbles; subjecting the tobacco extract from which the precipitate has been removed, to a fractionation operation using an ultrafiltration membrane or a reverse osmosis membrane to obtain both a first fraction which contains the desired components and in which the content of the undesired components has been rendered low and a second fraction in which the content of the desired components has been rendered low and the content of the undesired components has been rendered high; preparing a regenerated-tobacco web which contains the extraction residue; and adding the first fraction to the regenerated-tobacco web.

Description

再生タバコ材の製造方法および装置Method and apparatus for producing recycled tobacco material
　本発明は、再生タバコ材の製造方法およびその製造方法に用いられる装置に関する。 The present invention relates to a method for producing a recycled tobacco material and an apparatus used for the method.
　天然のタバコの葉、刻、中骨、茎、根等のタバコ材には、ニコチン、硝酸塩類、ニトロソアミン類、炭化水素類、蛋白質等種々の成分が含まれている。天然のタバコ材からこれら成分を抽出し、タバコへの喫味添加剤として使用することが行われている。その際、喫味または他の理由から、その量を減少させるか、除去することが望ましい成分（不所望成分）がある一方、除去しないかあるいはその濃度を増加させる方が望ましい成分（所望成分）もある。所望成分には、アミノ酸、糖類、ニコチン、葉面樹脂、アルカロイド類が含まれ、不所望成分には、硝酸塩、タバコ特異的ニトロソアミン（ＴＳＮＡ）のようなニトロソアミン類が含まれる。 Tobacco materials such as natural tobacco leaves, chops, bones, stems and roots contain various components such as nicotine, nitrates, nitrosamines, hydrocarbons and proteins. Extracting these components from natural tobacco materials and using them as a taste additive for tobacco has been carried out. In that case, there is a component that is desired to be reduced or removed (undesirable component) for taste or for other reasons, while another component (desired component) that is desired not to be removed or increased in concentration is also desired. is there. Desired components include amino acids, sugars, nicotine, foliar resins, alkaloids, and undesired components include nitrates and nitrosamines such as tobacco specific nitrosamine (TSNA).
　特許文献１は、天然のタバコ材を抽出し、タバコ抽出液と抽出残渣を獲得し、タバコ抽出液を、限外ろ過膜もしくは逆浸透ろ過膜（これらを総称して分画膜という）による膜分画操作に供して所望成分が富化され、かつ不所望成分が貧化された第１の画分と、所望成分が貧化され、かつ不所望成分が富化された第２の画分とを得ることを包含する再生タバコ材の製造方法を開示している。前記抽出残渣を用いて再生タバコウエブが調製され、このウエブに、前記第１の画分を添加することによって、再生タバコ材が製造される。 Patent Document 1 extracts a natural tobacco material, obtains a tobacco extract and an extraction residue, and converts the tobacco extract into a membrane using an ultrafiltration membrane or a reverse osmosis filtration membrane (collectively referred to as a fractionation membrane). A first fraction enriched with desired components and subjected to fractionation and subjected to fractionation, and a second fraction enriched with unwanted components and enriched with unwanted components A method for producing a recycled tobacco material is disclosed. A recycled tobacco web is prepared using the extraction residue, and a recycled tobacco material is produced by adding the first fraction to the web.
　特許文献１に開示された膜分画操作を連続して行うと、分画膜の表面にタバコ抽出液中に含まれる分画膜不透過成分等が付着して分画膜の分画性能や分画効率の低下を引き起こす。このような付着物質は、薬品による洗浄では効率的に除去することができない。また、タバコ抽出液中に含まれる糖や蛋白質は、タバコ抽出液を貯蔵容器に長期間貯蔵すると、タバコ抽出液から粒子状に析出し、分画膜を閉塞することが確認されている。 When the membrane fractionation operation disclosed in Patent Document 1 is carried out continuously, the fractionation performance of the fractionation membrane, such as the fractional membrane impermeable component contained in the tobacco extract adheres to the surface of the fractionation membrane, Causes a reduction in fractionation efficiency. Such adhered substances cannot be efficiently removed by cleaning with chemicals. In addition, it has been confirmed that sugars and proteins contained in the tobacco extract are deposited in a particulate form from the tobacco extract when the tobacco extract is stored in a storage container for a long period of time and clogs the fractionation membrane.
　特許文献２は、マイクロバブルやナノバブル等の微細気泡を含む処理液（分画膜によるろ過水または分画膜に供する原水を分画膜に接触させることにより、分画膜に付着した物質を除去することを開示している。 Patent Document 2 discloses a treatment liquid containing microbubbles such as microbubbles and nanobubbles (substances attached to a fractionation membrane are brought into contact with the fractionated membrane by bringing filtered water from the fractionation membrane or raw water supplied to the fractionation membrane into contact with the fractionation membrane. Is disclosed.
　しかしながら、タバコ抽出液は、糖や蛋白質を比較的多量に含み、これを分画膜による分画操作に供する場合、マイクロバブルやナノバブルを含む処理液による洗浄では、付着物質が十分に除去され得ない。 However, tobacco extract contains a relatively large amount of sugar and protein, and when it is subjected to fractionation using a fractionation membrane, washing with a treatment liquid containing microbubbles and nanobubbles can sufficiently remove the adhered substances. Absent.
米国特許第７６７７２５３号明細書US Pat. No. 7,677,253 日本国特開２０１０－２５３４５７Japan 2010-253457
　本発明は、分画膜（限外ろ過膜または逆浸透膜）によるタバコ抽出液中の所望成分と不所望成分との分離を連続的かつ効率的に行うことを可能とし、もって有意量の所望成分を含有するが、不所望成分の量が有意に低下した再生タバコ材を製造する方法を提供することを目的とする。 The present invention enables continuous and efficient separation of desired and undesired components in tobacco extract by a fractionation membrane (ultrafiltration membrane or reverse osmosis membrane). It is an object to provide a method for producing a regenerated tobacco material that contains components but has a significantly reduced amount of undesired components.
　また、本発明は、分画膜を用いて、タバコ抽出液から、有意量の所望成分を含有するが、不所望成分の量が有意に除去された画分を連続的かつ効率的に得るための装置を提供することを目的とする。 In addition, the present invention provides a fractionation membrane for continuously and efficiently obtaining a fraction containing a significant amount of a desired component but a significant amount of an undesirable component removed from a tobacco extract. An object of the present invention is to provide a device.
　本発明の一つの側面によると、（ａ）天然タバコ材を抽出溶媒で抽出して、所望成分と不所望成分とを含有するタバコ抽出液および抽出残渣を得ること、（ｂ）前記タバコ抽出液を、マイクロバブルと接触させること、（ｃ）マイクロバブルとの接触により前記タバコ抽出液中に析出した析出物を除去すること、（ｄ）前記析出物が除去されたタバコ抽出液を限外ろ過膜または逆浸透膜による分画操作に供して、前記所望成分を含有し、かつ前記不所望成分が貧化された第１の画分と、前記所望成分が貧化され、かつ前記不所望成分が富化された第２の画分とを得ること、（ｅ）前記抽出残渣を含む再生タバコウエブを調製すること、および（ｆ）前記第１の画分を前記再生タバコウエブに添加することを包含する再生タバコ材の製造方法が提供される。 According to one aspect of the present invention, (a) a natural tobacco material is extracted with an extraction solvent to obtain a tobacco extract containing the desired and undesired components and an extraction residue, and (b) the tobacco extract. (C) removing precipitates deposited in the tobacco extract by contact with the microbubbles; (d) ultrafiltration of the tobacco extract from which the deposits have been removed. A first fraction containing the desired component and having the undesired component deteriorated by being subjected to a fractionation operation using a membrane or a reverse osmosis membrane; And (e) preparing a regenerated tobacco web containing the extraction residue, and (f) adding the first fraction to the regenerated tobacco web. For producing recycled tobacco material including It is provided.
　また、本発明の他の側面によると、タバコ抽出液中の所望成分と不所望成分とを分離するための分画装置であって、タバコ抽出液を収容する第１の容器と、マイクロバブル発生装置と、前記発生したマイクロバブルを、該マイクロバブルで前記タバコ抽出液を処理して前記タバコ抽出液から析出物を析出させるために、前記第１の容器に送給する第１の送給デバイス（例えば、ポンプ）と、前記マイクロバブルで処理されたタバコ抽出液を、前記所望成分を含有し、かつ前記不所望成分が貧化された第１の画分と、前記所望成分が貧化され、かつ前記不所望成分が富化された第２の画分とに分画する限外ろ過膜または逆浸透膜を備える分画デバイスとを備える装置が提供される。 According to another aspect of the present invention, there is provided a fractionation device for separating a desired component and an undesired component in a tobacco extract, a first container containing a tobacco extract, and generation of microbubbles An apparatus and a first feeding device for feeding the generated microbubbles to the first container for treating the tobacco extract with the microbubbles to deposit precipitates from the tobacco extract (E.g., a pump), a tobacco extract treated with the microbubbles, a first fraction containing the desired component and the undesired component is degraded, and the desired component is degraded. And a fractionation device comprising an ultrafiltration membrane or a reverse osmosis membrane that fractionates into a second fraction enriched in the undesired components.
　本発明によると、限外ろ過膜または逆浸透膜によるタバコ抽出液中の所望成分と不所望成分との連続的かつ効率的な分離を可能にし、もって有意量の所望成分を含有するが、不所望成分が有意に低下した再生タバコ材を製造することができる。 The present invention allows continuous and efficient separation of desired and undesired components in tobacco extract by ultrafiltration membranes or reverse osmosis membranes, thus containing significant amounts of desired components but not Recycled tobacco materials with significantly reduced desired components can be produced.
図１は、本発明の一つの態様に係る分画装置の概略図である。FIG. 1 is a schematic diagram of a fractionation apparatus according to one embodiment of the present invention. 図２は、以後詳述する例１の結果を比較例の結果とともに示す図。FIG. 2 is a diagram showing the results of Example 1, which will be described in detail later, together with the results of a comparative example. 図３は、以後詳述する例１の結果を比較例の結果とともに示す図。FIG. 3 is a diagram showing the results of Example 1 described in detail below together with the results of Comparative Examples.
　本発明の一つの側面は、天然タバコ材を抽出することにより得られたタバコ抽出液と抽出残渣を用いて再生タバコ材を製造する方法に関する。一方で、抽出残渣を含む再生タバコウエブを製造する。他方で、タバコ抽出液を、マイクロバブルと接触させ、その接触の結果タバコ抽出液中に析出した析出物を除去する。析出物が除去されたタバコ抽出液を分画膜（限外ろ過膜または逆浸透膜）による分画操作に供する。この分画操作により、所望成分を含有し、不所望成分が貧化された第１の画分と、所望成分が貧化され、かつ不所望成分が富化された第２の画分とが得られる。第１の画分を再生タバコウエブに添加することによって所望の再生タバコ材が製造される。 One aspect of the present invention relates to a method for producing a regenerated tobacco material using a tobacco extract obtained by extracting a natural tobacco material and an extraction residue. On the other hand, the regenerated tobacco web containing the extraction residue is manufactured. On the other hand, the tobacco extract is brought into contact with the microbubbles, and deposits deposited in the tobacco extract as a result of the contact are removed. The tobacco extract from which the precipitate has been removed is subjected to a fractionation operation using a fractionation membrane (ultrafiltration membrane or reverse osmosis membrane). By this fractionation operation, a first fraction containing a desired component and an unwanted component is poored, and a second fraction in which the desired component is poored and the unwanted component is enriched can get. The desired regenerated tobacco material is produced by adding the first fraction to the regenerated tobacco web.
　より具体的には、まず、天然タバコ材と抽出溶媒を混合し、撹拌する。天然タバコ材としては、タバコの葉、その刻、中骨、茎、根およびそれらの混合物を用いることができる。抽出溶媒としては、水、または水と水混和性有機溶媒との混合物を使用することができる。水混和性有機溶媒の例を挙げると、エタノールのようなアルコール類、ジエチルエーテルのようなエーテル類等である。抽出処理は、通常、０～１００℃の温度で、５分～６時間行うことができる。 More specifically, first, the natural tobacco material and the extraction solvent are mixed and stirred. As the natural tobacco material, tobacco leaf, its chop, middle bone, stem, root and a mixture thereof can be used. As the extraction solvent, water or a mixture of water and a water-miscible organic solvent can be used. Examples of water-miscible organic solvents are alcohols such as ethanol, ethers such as diethyl ether, and the like. The extraction treatment can usually be performed at a temperature of 0 to 100 ° C. for 5 minutes to 6 hours.
　抽出処理の終了後、得られた抽出混合物を例えばろ過、遠心分離等による分離操作に供し、タバコ抽出液と抽出残渣に分ける。 After completion of the extraction treatment, the obtained extraction mixture is subjected to a separation operation such as filtration, centrifugation, etc., and separated into tobacco extract and extraction residue.
　天然タバコ材には、カリウム等の金属の塩、硝酸塩、ニコチン、ショ糖等の糖類、アミノ酸類、配糖体、アミノ－糖化合物類、蛋白質、炭化水素類（飽和炭化水素類、不飽和炭化水素類、芳香族炭化水素類）、アルコール類、エーテル類、アルデヒド類、ケトン類、エステル類、ラクトン類、キノン類、酸類（酸無水物を含む）、フェノール類、アミン類、ピロール類、ピリジン類、ピラジン類、アルカロイド類、多環式含窒素化合物類、ニトロソアミン（ＴＳＮＡを含む）等のニトロソ化合物類、アミド類、脂質類、ハロゲン化物、含硫黄化合物、無機元素等が含まれる。上記抽出処理により得られるタバコ抽出液には、使用する抽出溶媒の種類にもよるが、これら成分のほとんどが含まれ得る。これら成分のうち、所望成分には、アミノ酸、糖類、ニコチン、葉面樹脂、アルカロイド類が含まれ、不所望成分には、硝酸塩、ＴＳＮＡのようなニトロソアミン類が含まれる。ＴＳＮＡの代表例は、ニトロソアミン（Ｎ’－ニトロソノルニコチン（ＮＮＮ）、４－（メチルニトロソアミノ）－１－（３－ピリジル）－１－ブタノン（ＮＮＫ）、Ｎ’－ニトロソアナタビン（ＮＡＴ）、Ｎ’－ニトロソアナバシン（ＮＡＢ）である。 Natural tobacco materials include metal salts such as potassium, nitrates, nicotine, sugars such as sucrose, amino acids, glycosides, amino-sugar compounds, proteins, hydrocarbons (saturated hydrocarbons, unsaturated carbonization) Hydrogen, aromatic hydrocarbons), alcohols, ethers, aldehydes, ketones, esters, lactones, quinones, acids (including acid anhydrides), phenols, amines, pyrroles, pyridine , So-called pyrazines, alkaloids, polycyclic nitrogen-containing compounds, nitroso compounds such as nitrosamines (including TSNA), amides, lipids, halides, sulfur-containing compounds, inorganic elements and the like. The tobacco extract obtained by the extraction treatment can contain most of these components, although depending on the type of extraction solvent used. Among these components, desired components include amino acids, sugars, nicotine, foliar resin, and alkaloids, and undesired components include nitrosamines such as nitrates and TSNA. Representative examples of TSNA are nitrosamines (N′-nitrosonornicotine (NNN), 4- (methylnitrosoamino) -1- (3-pyridyl) -1-butanone (NNK), N′-nitrosoanatabine (NAT) N′-nitrosoanabasin (NAB).
　前記抽出残渣は、抽出溶媒に不溶性の成分であり、実質的に繊維からなる。この抽出残渣を用いて、常法により、再生タバコウエブを製造する。この再生タバコウエブは、その一部が抽出残渣により構成されるものでもよいし、その全部が抽出残渣により構成されるものでもよい。例えば、抽出残渣を含むパルプ材を通常の抄紙工程で抄紙して再生タバコウエブとすることができる。 The extraction residue is a component that is insoluble in the extraction solvent and substantially consists of fibers. Using this extraction residue, a regenerated tobacco web is produced by a conventional method. A part of the regenerated tobacco web may be constituted by an extraction residue, or the whole may be constituted by an extraction residue. For example, a pulp material containing an extraction residue can be made into a recycled tobacco web by paper making in a normal paper making process.
　他方、前記タバコ抽出液（以下、「原液」ということがある）を、原液容器に収容し、マイクロバブル発生装置により発生したマイクロバブルと接触させる。マイクロバブルの発生機構および発生装置は、当該分野でよく知られており、ここでは述べない。マイクロバブル発生装置は、市販されている。マイクロバブルは、原液を用いて発生させることもできるし、後に記載する分画膜により分画された膜透過物もしくは膜不透過物を用いて発生させることもできる。マイクロバブルは、０．０００００５ｍｍ～０．１ｍｍの直径を有し得る。マイクロバブルを原液容器に導入し、マイクロバブルによる前処理を行うことができる。タバコ抽出液をマイクロバブルと接触させると、タバコ抽出液中に含まれていた糖類、油脂類、蛋白質等が析出し、原液表面に浮遊してくる。これら浮遊する析出物は、マイクロバブルで前処理した原液は以後述べるように通常原液容器の底部から前処理済液容器に送るので、すぐに取り除く必要はなく、ある程度の量がたまったら、柄杓等で掬い取るか、金属もしくは紙フィルタで除去することができる。すなわち、本発明において、析出物の除去は、析出物が原液表面に浮遊する結果、析出物が原液から分離されることを含む。 On the other hand, the tobacco extract (hereinafter sometimes referred to as “stock solution”) is contained in a stock solution container and brought into contact with microbubbles generated by a microbubble generator. Microbubble generation mechanisms and generators are well known in the art and will not be described here. Microbubble generators are commercially available. Microbubbles can be generated using a stock solution, or can be generated using a membrane permeate or a membrane impermeate fractionated by a fractionation membrane described later. The microbubbles can have a diameter of 0.000005 mm to 0.1 mm. Microbubbles can be introduced into a stock solution container and pretreatment with microbubbles can be performed. When the tobacco extract is brought into contact with the microbubbles, sugars, fats, proteins, etc. contained in the tobacco extract are precipitated and float on the surface of the stock solution. These floating precipitates are usually sent from the bottom of the stock solution container to the pretreated solution container as described below, so that the stock solution pretreated with microbubbles does not need to be removed immediately. Can be scraped off or removed with a metal or paper filter. That is, in the present invention, the removal of the precipitate includes that the precipitate is separated from the stock solution as a result of the precipitate floating on the surface of the stock solution.
　析出物を除去したタバコ抽出液を１バッチ量、前処理済液容器に収容し、そこから分画膜に送り、分画膜による分画操作に供して、膜透過物画分と、膜不透過物画分とに分画する。 A batch of tobacco extract from which precipitates have been removed is stored in a pre-treated liquid container, sent from there to a fractionation membrane, and subjected to fractionation operation with a fractionation membrane to give a membrane permeate fraction and a membrane-free fraction. Fractionate into permeate fraction.
　分画膜として逆浸透膜を用いた場合、膜透過物画分は、ＴＳＮＡを含む不所望成分が富化されている。対応して、膜不透過物画分は、ＴＳＮＡ等を含む不所望成分が貧化されている。膜不透過物画分は、タバコ抽出液中の所望成分（例えばニコチン）の初期量を実質的に（８５重量％以上）維持することができ、対応して、膜透過物画分は所望成分を実質的に含まない。逆浸透膜としては、上記不所望成分透過させるが、上記所望成分を実質的に透過させないものである。逆浸透膜は、タバコ抽出液中の糖分等の可溶性成分（ＴＳＮＡを除く）を透過させないものであることが好ましい。逆浸透膜としては、孔径０．１～３ｎｍのものを用いることができる。逆浸透膜は、平膜であっても、袋状のものを筒状に成形したもの（スパイラル膜）であって、あるいは中空糸膜またはチューブラ膜であってもよい。タバコ抽出液は、例えば、１～３ＭＰａの圧力で逆浸透膜に供給することができる。タバコ抽出液の逆浸透膜への供給は、高圧ポンプを用いて行うことができる。 When a reverse osmosis membrane is used as the fractionation membrane, the membrane permeate fraction is enriched with undesirable components including TSNA. Correspondingly, the membrane impermeate fraction is poor in unwanted components including TSNA. The membrane-impermeable fraction can substantially maintain the initial amount of desired component (eg nicotine) in the tobacco extract (85% by weight or more), correspondingly the membrane-permeate fraction Is substantially not included. The reverse osmosis membrane allows the undesired component to permeate but does not substantially permeate the desired component. The reverse osmosis membrane is preferably one that does not allow permeation of soluble components (excluding TSNA) such as sugar in the tobacco extract. A reverse osmosis membrane having a pore diameter of 0.1 to 3 nm can be used. The reverse osmosis membrane may be a flat membrane, a bag-shaped one formed into a cylindrical shape (spiral membrane), or a hollow fiber membrane or a tubular membrane. For example, the tobacco extract can be supplied to the reverse osmosis membrane at a pressure of 1 to 3 MPa. The tobacco extract can be supplied to the reverse osmosis membrane using a high-pressure pump.
　他方、分画膜として限外ろ過膜を用いた場合、膜不透過物画分は、不所望成分が富化され、膜透過物画分は、対応して、不所望成分が貧化されている。限外ろ過膜の分画分子量の範囲は、１，０００から１，０００，０００までである。 On the other hand, when an ultrafiltration membrane is used as a fractionation membrane, the membrane impermeate fraction is enriched with unwanted components, and the membrane permeate fraction is correspondingly enriched with unwanted components. Yes. The range of the molecular weight cut off of the ultrafiltration membrane is 1,000 to 1,000,000.
　不所望成分が富化された画分は廃棄する。 画 Discard fractions enriched with unwanted components.
　不所望成分が貧化された画分を前処理済液容器に戻し、再び分画膜に送り、分画操作を行うことができる。この分画操作を、不所望成分、例えばＴＳＮＡの量が、初期量の例えば約４０重量％以下（ＴＳＮＡ除去率６０重量％以上）、あるいは２０重量％以下（ＴＳＮＡ除去率８０重量％以上）、さらには１０重量％以下（ＴＳＮＡ除去率９０重量％以上）となるまで繰り返し行うことができる。所望成分（例えばニコチン）は、初期量の８５重量％以上が維持され得る。 The fraction in which the undesirable components are deteriorated can be returned to the pretreated liquid container and sent again to the fractionation membrane to perform the fractionation operation. In this fractionation operation, the amount of undesired components such as TSNA is, for example, about 40% by weight or less of the initial amount (TSNA removal rate of 60% by weight or more), or 20% by weight or less (TSNA removal rate of 80% by weight or more), Further, the process can be repeated until it is 10% by weight or less (TSNA removal rate is 90% by weight or more). The desired component (eg, nicotine) can be maintained at 85% or more of the initial amount.
　こうして１バッチ量のタバコ抽出液を分画処理した後、次のバッチのタバコ抽出液について同様の分画操作をおこなう。このような分画操作を複数バッチ量のタバコ抽出液について連続的に繰り返した後、分画操作を停止し、分画膜の洗浄を行うことが好ましい。この分画膜の洗浄は、水をマイクロバブル発生装置に通じて得られたマイクロバブル含有水（洗浄液）を用いて行うことができる。この洗浄液を前処理液容器に収容し、そこから分画膜に送り、分画膜を洗浄する。洗浄液の膜透過物および膜不透過物は前処理液容器に戻し、洗浄液を再びマイクロバブル発生装置に送り、得られたマイクロバブルを含む処理液（洗浄液）を再び前記前処理液貯蔵容器に送る一方、前記前処理液貯蔵容器から処理液（洗浄液）を分画膜に送り、これを洗浄する。このような洗浄サイクルを所定時間繰り返した後、洗浄操作を停止し、タバコ抽出液の分画操作を再開始する。 Thus, after fractionating one batch of tobacco extract, the same fractionation operation is performed on the next batch of tobacco extract. It is preferable that such a fractionation operation is continuously repeated for a plurality of batches of tobacco extract, then the fractionation operation is stopped and the fractionation membrane is washed. This fractionation membrane can be washed using water containing microbubbles (cleaning solution) obtained by passing water through a microbubble generator. This cleaning liquid is accommodated in a pretreatment liquid container, and sent from there to the fractionation membrane to wash the fractionation membrane. The membrane permeate and membrane impermeate of the cleaning liquid are returned to the pretreatment liquid container, the cleaning liquid is sent again to the microbubble generator, and the obtained processing liquid (cleaning liquid) containing the microbubbles is sent again to the pretreatment liquid storage container. On the other hand, the treatment liquid (cleaning liquid) is sent from the pretreatment liquid storage container to the fractionation membrane and washed. After such a washing cycle is repeated for a predetermined time, the washing operation is stopped and the tobacco extract liquid fractionation operation is restarted.
　上記洗浄に際しては、マイクロバブルを含む洗浄液にオゾンを導入することができる。オゾンは、オゾン発生器から発生させ、洗浄のために前処理液貯蔵装置から分画膜に向かう洗浄液としての前処理液中に導入することができる。このオゾン処理により、分画膜の洗浄効率が一層向上する。 In the above cleaning, ozone can be introduced into the cleaning liquid containing microbubbles. Ozone can be generated from an ozone generator and introduced into a pretreatment liquid as a cleaning liquid from the pretreatment liquid storage device toward the fractionation membrane for cleaning. This ozone treatment further improves the cleaning efficiency of the fractionation film.
　また、オゾンを含むことのある洗浄液による洗浄処理の前および／または後に、分画膜を温水（温度４０～１００℃）および／またはアルカリ水溶液（例えば、水酸化ナトリウム水溶液、あるいはラウリル硫酸ナトリウム等のアルカリ性界面活性剤の水溶液）で洗浄することもできる。 In addition, before and / or after the cleaning treatment with a cleaning solution that may contain ozone, the separation membrane may be heated with warm water (temperature 40 to 100 ° C.) and / or an alkaline aqueous solution (for example, sodium hydroxide aqueous solution or sodium lauryl sulfate). It can also be washed with an aqueous solution of an alkaline surfactant.
　図１は、本発明の一つの態様に係る分画装置１０の概略図であり、分画膜として逆浸透膜を備える態様について説明する。図１に示す分画装置１０は、前記天然タバコ剤の抽出処理により得られ抽出液（原液）ＴＥＬを収容する容器１１１、マイクロバブルによる前処理済タバコ抽出液ＴＴＥを収容するための容器１１２、マイクロバブル発生装置１１３、および分画膜１１４１を備える分画デバイス１１４を具備する。以下の記述において上流、下流は、液の流れ方向を基準とする。 FIG. 1 is a schematic diagram of a fractionation apparatus 10 according to one aspect of the present invention, and an aspect having a reverse osmosis membrane as a fractionation membrane will be described. A fractionation device 10 shown in FIG. 1 includes a container 111 for storing an extract (stock solution) TEL obtained by the extraction process of the natural tobacco agent, a container 112 for storing a pretreated tobacco extract TTE by microbubbles, A microbubble generator 113 and a fractionation device 114 including a fractionation film 1141 are provided. In the following description, upstream and downstream are based on the liquid flow direction.
　ＴＥＬ容器１１１の底部は、開閉弁Ｖ１を備えるラインＬ１を介してポンプＰ１の入口に連通し、ポンプＰ１の出口は、ラインＬ２を介してマイクロバブル発生装置１１３の入口に連通する。開閉弁Ｖ２を備えるラインＬ３が、マイクロバブル発生装置１１３の出口とＴＥＬ容器１１１の頂部を連通させている。 The bottom of the TEL container 111 communicates with the inlet of the pump P1 through a line L1 having an on-off valve V1, and the outlet of the pump P1 communicates with the inlet of the microbubble generator 113 through a line L2. A line L3 including the on-off valve V2 communicates the outlet of the microbubble generator 113 and the top of the TEL container 111.
　ＴＥＬ容器１１１の底部は、開閉弁Ｖ３を備えるラインＬ４を介して、ポンプＰ２の入口に連通し、ポンプＰ２の出口は、ラインＬ５を介してＴＴＥ容器１１２の頂部に連通する。 The bottom of the TEL container 111 communicates with the inlet of the pump P2 via a line L4 having an on-off valve V3, and the outlet of the pump P2 communicates with the top of the TTE container 112 via a line L5.
　ＴＴＥ容器１１２の底部は、開閉弁Ｖ４を備えるラインＬ６を介してポンプＰ３の入口に連通し、ポンプＰ３の出口は、開閉弁Ｖ５を備えるラインＬ７を介して、分画デバイス１１４の入口に連通する。 The bottom of the TTE container 112 communicates with the inlet of the pump P3 via a line L6 provided with the on-off valve V4, and the outlet of the pump P3 communicates with the inlet of the fractionation device 114 via the line L7 provided with the on-off valve V5. To do.
　分画デバイス１１４の膜不透過物出口は、開閉弁Ｖ６を備えるラインＬ８を介してＴＴＥ容器１１２の頂部に連通する。分画デバイス１１４の膜透過物出口は、開閉弁Ｖ７を備える廃棄ラインＬ９に接続されている。 The membrane impermeate outlet of the fractionation device 114 communicates with the top of the TTE container 112 via a line L8 having an on-off valve V6. The membrane permeate outlet of the fractionation device 114 is connected to a waste line L9 including an on-off valve V7.
　本発明の一つの態様において、開閉弁Ｖ３、Ｖ４およびＶ５を閉じるとともに開閉弁Ｖ１およびＶ２を開き、ポンプＰ１を駆動することにより、ＴＥＬ容器１１１中の原液（タバコ抽出液）をラインＬ１およびラインＬ２を介してマイクロバブル発生装置１１３に導入し、マイクロバブル発生装置１１３でマイクロバブルを発生させ、そのマイクロバブルを含むタバコ抽出液（前処理液）を、ラインＬ３を介してＴＥＬ容器１１１中の原液中に供給する。ＴＥＬ容器１１１においてマイクロバブルと接触した結果、原液中に含まれていた糖類、油脂類、タンパク質等の分画膜閉塞物質が原液から析出し、原液表面に浮遊する。この浮遊物の処置については上に述べた。ついで開閉弁Ｖ１を閉じ、ポンプＰ１の作動を停止するとともに、開閉弁Ｖ３を開き、ポンプＰ２を駆動することにより、容器１１１中の前処理済原液を１バッチ量（例えば、１０～１００Ｌ）、ラインＬ４およびＬ５を介してＴＴＥ容器１１２に導入する。導入後、開閉弁Ｖ３を閉じ、ポンプＰ２の作動を停止するとともに、開閉弁Ｖ４～Ｖ７を開き、ポンプＰ３を駆動することにより、前処理済タバコ抽出液をＴＴＥ容器１１２から分画デバイス１１４に順次供給する。分画デバイス１１４においては、分画膜（本態様では逆浸透膜）１１４１により、前処理済タバコ抽出液を、所望成分を含み、ＴＳＮＡ等の不所望成分が貧化された膜不透過物画分と、所望成分が貧化され、ＴＳＮＡ等の不所望成分が富化された膜透過物画分とに分画する。膜不透過物画分はラインＬ８を介してＴＴＥ容器１１２に戻す一方、膜透過物画分は、ラインＬ９を介して廃棄する。この分画操作を、膜不透過物画分中の不所望成分、例えばＴＳＮＡの量が、初期量の例えば約４０重量％以下（ＴＳＮＡ除去率６０重量％以上）、あるいは２０重量％以下（ＴＳＮＡ除去率８０重量％以上）、さらには１０重量％以下（ＴＳＮＡ除去率９０重量％以上）となるまで繰り返し行うことができる。所望成分（例えばニコチン）は、初期量の８５重量％以上が維持され得る。膜不透過物画分は、繰り返しの分画操作により順次濃縮してゆく。膜不透過物中の不所望成分の量は、例えば、廃棄した膜透過物画分中のＴＳＮＡの量を測定することにより知ることができる。こうして１バッチ量のタバコ抽出液を分画処理した後、ＴＴＥ容器１１２に収容された濃縮タバコ抽出液を回収する。ついで、上に述べたように、ＴＥＬ容器１１１からＴＴＥ容器１１２に、次の１バッチ量の前処理済タバコ抽出液を導入し、同様の分画操作を行う。本発明において、タバコ抽出液（原液）は、マイクロバルブによる前処理により分画膜閉塞物質が除去されているので、そのような前処理を行わない場合に比べて、分画膜における初期流速に対する透過流束の低下が５０％以下に抑えられ、連続分画処理時間が有意に延長する。このようにしてタバコ抽出液のバッチ式分画操作を複数回繰り返した後、分画操作を停止し、分画膜の洗浄を行うことが好ましい。 In one embodiment of the present invention, the on-off valves V3, V4 and V5 are closed, the on-off valves V1 and V2 are opened, and the pump P1 is driven, whereby the stock solution (tobacco extract) in the TEL container 111 is supplied to the line L1 and the line. L2 is introduced into the microbubble generator 113, microbubbles are generated by the microbubble generator 113, and the tobacco extract (pretreatment liquid) containing the microbubbles is transferred to the TEL container 111 via the line L3. Supply into the stock solution. As a result of the contact with the microbubbles in the TEL container 111, the separation membrane blocking substances such as saccharides, fats and proteins contained in the stock solution are precipitated from the stock solution and float on the surface of the stock solution. The treatment of this floating substance was described above. Next, the on-off valve V1 is closed, the operation of the pump P1 is stopped, the on-off valve V3 is opened, and the pump P2 is driven, whereby one batch of pretreated stock solution in the container 111 (for example, 10 to 100 L), It introduces into the TTE container 112 via lines L4 and L5. After the introduction, the on-off valve V3 is closed, the operation of the pump P2 is stopped, the on-off valves V4 to V7 are opened, and the pump P3 is driven, whereby the pretreated tobacco extract is transferred from the TTE container 112 to the fractionation device 114. Supply sequentially. In the fractionation device 114, the membrane impermeate fraction containing the desired component and the unwanted component such as TSNA being deteriorated by the fractionated membrane (reverse osmosis membrane in this embodiment) 1141. And a membrane permeate fraction enriched with undesired components such as TSNA. The membrane-impermeable fraction is returned to the TTE vessel 112 via line L8, while the membrane-permeate fraction is discarded via line L9. In this fractionation operation, the amount of undesired components such as TSNA in the membrane-impermeable product fraction is, for example, about 40% by weight or less of the initial amount (TSNA removal rate of 60% by weight or more), or 20% by weight or less (TSNA). The removal can be repeated until the removal rate is 80% by weight or more, and further 10% by weight or less (the TSNA removal rate is 90% by weight or more). The desired component (eg, nicotine) can be maintained at 85% or more of the initial amount. The membrane-impermeable fraction is successively concentrated by repeated fractionation operations. The amount of undesired components in the membrane-impermeable material can be known, for example, by measuring the amount of TSNA in the discarded membrane-permeated fraction. After fractionating the batch of tobacco extract in this manner, the concentrated tobacco extract contained in the TTE container 112 is recovered. Then, as described above, the next batch of pretreated tobacco extract is introduced from the TEL container 111 to the TTE container 112, and the same fractionation operation is performed. In the present invention, the cigarette extract (stock solution) has been removed from the membrane occluding substance by pretreatment with a microvalve, so that compared to the case where such pretreatment is not performed, The decrease in permeation flux is suppressed to 50% or less, and the continuous fractionation processing time is significantly extended. Thus, it is preferable to stop the fractionation operation and wash the fractionation membrane after repeating the batch-type fractionation operation of the tobacco extract a plurality of times.
　したがって、本発明の好ましい態様において、分画装置１０は、洗浄機構を備える。より具体的には、図１に示すように、分画装置１０は、マイクロバブル含有液ＭＢＬを収容する容器１１５をさらに備える。ＭＢＬ容器１１５の底部に連通し、開閉弁Ｖ８を有するラインＬ１０が開閉弁Ｖ１の下流でラインＬ１に接続している。また、ＭＢＬ容器１１５の底部は、開閉弁Ｖ９を備えるラインＬ１１を介してポンプＰ３の入口に連通している。ポンプＰ３の出口に連通するラインＬ１２が、開閉弁Ｖ５の下流でラインＬ７に接続している。さらに、ＭＢＬ容器１１５の頂部に連通し、開閉弁Ｖ１０を備えるラインＬ１３が開閉弁Ｖ６の上流でラインＬ８に接続している。また、開閉弁Ｖ７の上流でラインＬ９から分岐し、開閉弁Ｖ１１を備えるラインＬ１４がＭＢＬ容器１１５の頂部に連通している。さらに、ＭＢＬ容器１１５の頂部に連通し、開閉弁Ｖ１２を備えるラインＬ１５がラインＬ３に接続している。 Therefore, in a preferred embodiment of the present invention, the fractionation device 10 includes a cleaning mechanism. More specifically, as shown in FIG. 1, the fractionation device 10 further includes a container 115 that stores the microbubble-containing liquid MBL. A line L10 that communicates with the bottom of the MBL container 115 and has an on-off valve V8 is connected to the line L1 downstream of the on-off valve V1. Further, the bottom of the MBL container 115 communicates with the inlet of the pump P3 via a line L11 having an on-off valve V9. A line L12 communicating with the outlet of the pump P3 is connected to the line L7 downstream of the on-off valve V5. Further, a line L13 that communicates with the top of the MBL container 115 and includes the on-off valve V10 is connected to the line L8 upstream of the on-off valve V6. In addition, a line L14 that branches from the line L9 upstream of the on-off valve V7 and communicates with the top of the MBL container 115. The line L14 includes the on-off valve V11. Further, a line L15 that communicates with the top of the MBL container 115 and includes an on-off valve V12 is connected to the line L3.
　分画装置１０は、オゾン発生器１１６を備えることが好ましい。オゾン発生器１１６は、開閉弁Ｖ１３を備えるラインＬ１６を介して、開閉弁Ｖ１の下流でラインＬ１に接続している。 The fractionation device 10 preferably includes an ozone generator 116. The ozone generator 116 is connected to the line L1 downstream of the on-off valve V1 via a line L16 provided with the on-off valve V13.
　分画膜１１４１の洗浄に際し、開閉弁Ｖ２、Ｖ８およびＶ９を閉じた状態で、まず、ＭＢＬ容器１１５に水を導入する。次に、開閉弁Ｖ８、Ｖ１２を開いた状態で、ポンプＰ１を駆動し、ＭＢＬ容器１１５中の水を、ラインＬ１０、Ｌ２を介してマイクロバブル発生装置１１３に送り、そこで得られたマイクロバブル含有水（洗浄液）をラインＬ１５を介してＭＢＬ容器１１５に導入する。この操作を繰り返し、一定量のマイクロバブル含有原液がＭＢＬ容器１１５に導入されたら、開閉弁Ｖ８を閉じ、開閉弁Ｖ９を開き、ポンプＰ３を駆動させて、ＭＢＬ容器１１５からマイクロバブル含有水（洗浄液）をラインＬ１２およびＬ７を介して分画デバイス１１４に送り、分画膜１１４１の洗浄を所定時間行う。マイクロバブルは、分画膜１１４１に付着した膜閉塞物質を除去する。この洗浄操作において、開閉弁Ｖ１３を開き、洗浄液に、オゾン発生器１１６からオゾンを導入すると、洗浄効率が一層向上する。洗浄液の不膜透過物画分は、ラインＬ８およびＬ１３を介してＭＢＬ容器１１５に導入する一方、洗浄液の膜透過物画分もラインＬ９およびＬ１４を介してＭＢＬ容器１１５に導入する。洗浄操作の終了後、上記手順に従って、タバコ抽出液の分画操作を再開始する。 When washing the separation membrane 1141, water is first introduced into the MBL container 115 with the on-off valves V2, V8 and V9 closed. Next, with the on-off valves V8 and V12 opened, the pump P1 is driven, and the water in the MBL container 115 is sent to the microbubble generator 113 through the lines L10 and L2, and the microbubbles contained therein are obtained. Water (cleaning liquid) is introduced into the MBL container 115 via the line L15. This operation is repeated, and when a certain amount of the microbubble-containing stock solution is introduced into the MBL container 115, the on-off valve V8 is closed, the on-off valve V9 is opened, and the pump P3 is driven to remove the microbubble-containing water (cleaning liquid) from the MBL container 115. ) Is sent to the fractionation device 114 via the lines L12 and L7, and the fractionation film 1141 is washed for a predetermined time. The microbubbles remove the membrane occluding substance adhering to the fractionation membrane 1141. In this cleaning operation, when the on-off valve V13 is opened and ozone is introduced into the cleaning liquid from the ozone generator 116, the cleaning efficiency is further improved. The non-membrane permeate fraction of the cleaning liquid is introduced into the MBL container 115 via lines L8 and L13, while the membrane permeate fraction of the cleaning liquid is also introduced into the MBL container 115 via lines L9 and L14. After completion of the washing operation, the tobacco extract solution fractionation operation is restarted according to the above procedure.
　本発明において、分画膜のマイクロバブルによる洗浄に加えて、分画膜を温水および／またはアルカリ水溶液で洗浄することができる。そのために、図１に示す分画装置１０は、図１に示すように、温水ＷＷを収容するＷＷ容器１１７および／またはアルカリ水溶液ＡＬを収容するＡＬ容器１１８を備える。ＷＷ容器１１７の底部に連通し、開閉弁Ｖ１４を備えるラインＬ１７が、開閉弁Ｖ４の下流でラインＬ６に接続している。また、ＡＬ容器１１８の底部に連通し、開閉弁Ｖ１５を備えるラインＬ１８が（図１に示す例では、ラインＬ１７を介して）ラインＬ６に接続している。ＷＷ容器１１７の頂部に連通し、開閉弁Ｖ１６を備えるライン１９が、開閉弁Ｖ１１の下流で、ラインＬ１４から分岐している。また、ＡＬ容器１１８の頂部に連通し、開閉弁Ｖ１７を備えるラインＬ２０が、開閉弁Ｖ１１の下流で、ラインＬ１４から分岐している。加えて、ＷＷ容器１１７の頂部に連通し、開閉弁Ｖ１８を備えるラインＬ２１が、開閉弁Ｖ６の上流で、ラインＬ８から分岐している。また、ＡＬ容器１１８の頂部に連通し、開閉弁Ｖ１９を備えるラインＬ２２が、開閉弁Ｖ６の上流で、ラインＬ８から分岐している。 In the present invention, in addition to washing the membrane with microbubbles, the membrane can be washed with warm water and / or an alkaline aqueous solution. For this purpose, the fractionation device 10 shown in FIG. 1 includes a WW container 117 for containing hot water WW and / or an AL container 118 for containing an alkaline aqueous solution AL, as shown in FIG. A line L17 that communicates with the bottom of the WW container 117 and includes the on-off valve V14 is connected to the line L6 downstream of the on-off valve V4. Further, a line L18 that communicates with the bottom of the AL container 118 and includes an on-off valve V15 is connected to the line L6 (via the line L17 in the example shown in FIG. 1). A line 19 that communicates with the top of the WW container 117 and includes an on-off valve V16 branches off from the line L14 downstream of the on-off valve V11. A line L20 that communicates with the top of the AL container 118 and includes the on-off valve V17 branches from the line L14 downstream of the on-off valve V11. In addition, a line L21 that communicates with the top of the WW container 117 and includes the on-off valve V18 branches from the line L8 upstream of the on-off valve V6. A line L22 that communicates with the top of the AL container 118 and includes the on-off valve V19 branches off from the line L8 upstream of the on-off valve V6.
　本発明において、分画膜の洗浄プロセスが、マイクロバブルによる洗浄に加えて、温水洗浄および／またはアルカリ水溶液洗浄を含む場合、これら２つまたは３つの洗浄工程の順番に特に制限はないが、通常、温水洗浄、マイクバブル洗浄およびアルカリ水溶液洗浄の順で行われる。その場合の洗浄プロセスを、念のため、図１を参照して以下説明する。 In the present invention, when the washing process of the fractionation membrane includes warm water washing and / or alkaline aqueous solution washing in addition to washing with microbubbles, the order of these two or three washing steps is not particularly limited. , Warm water cleaning, microphone bubble cleaning, and alkaline aqueous solution cleaning. The cleaning process in that case will be described below with reference to FIG. 1 just in case.
　タバコ抽出液の分画操作は終了しているので、開閉弁Ｖ４、Ｖ５、Ｖ６およびＶ７を閉じ、ポンプＰ３の作動を停止する。そして、開閉弁Ｖ８、Ｖ９、Ｖ１０、Ｖ１２、Ｖ１３、Ｖ１５、Ｖ１７、Ｖ１９も閉じ、開閉弁Ｖ１４、Ｖ１６およびＶ１８を開き、ポンプＰ３を駆動し、温水ＷＷをＷＷ容器１１７から、ラインＬ１７、Ｌ６およびＬ７を介して分画デバイス１１４に導入し、分画膜１１４１を洗浄する。温水の膜不透過物はラインＬ８およびＬ２１を介してＷＷ容器１１７に戻す一方、温水の膜透過物もラインＬ１４およびＬ１９を介してＷＷ容器１１７に戻す。こうして温水による分画膜１１４１を洗浄したのち、開閉弁Ｖ１６およびＶ１８を閉じ、上に述べたように、好ましくはオゾンを含むマイクロバブル含有洗浄液で分画膜１１４１を洗浄する。その後、開閉弁Ｖ８、Ｖ９を閉じ、開閉弁Ｖ１５、Ｖ１７およびＶ１９を開き、アルカリ水溶液ＡＬをＡＬ容器１１８からラインＬ１８、Ｌ６およびＬ７を介して分画デバイス１１４に導入し、アルカリ水溶液ＡＬにより分画膜１１４１を洗浄する。アルカリ水溶液の膜不透過物は、ラインＬ８およびＬ２２を介してＡＬ容器１１８に戻す一方、アルカリ水溶液の膜透過物もラインＬ１４およびＬ２２を介してＡＬ容器１１８に戻す。こうして、分画膜１１４１の洗浄が終了したのち、上述の手法によりタバコ抽出液の分画操作を再開始する。 Since the fractionation operation of the tobacco extract has been completed, the on-off valves V4, V5, V6 and V7 are closed, and the operation of the pump P3 is stopped. And the on-off valves V8, V9, V10, V12, V13, V15, V17, V19 are also closed, the on-off valves V14, V16, and V18 are opened, the pump P3 is driven, and the hot water WW is supplied from the WW container 117 to the lines L17, L6. And introduced into the fractionation device 114 via L7, and the fractionation film 1141 is washed. The membrane permeate of warm water is returned to the WW container 117 via lines L8 and L21, while the membrane permeate of warm water is also returned to the WW container 117 via lines L14 and L19. After the membrane 1141 is washed with warm water in this way, the on-off valves V16 and V18 are closed, and the membrane 1141 is washed with a cleaning solution containing microbubbles preferably containing ozone as described above. Thereafter, the on-off valves V8 and V9 are closed, the on-off valves V15, V17 and V19 are opened, and the alkaline aqueous solution AL is introduced from the AL container 118 into the fractionation device 114 via the lines L18, L6 and L7. The image film 1141 is washed. The membrane-impermeable substance of the alkaline aqueous solution is returned to the AL container 118 via the lines L8 and L22, while the membrane-permeable substance of the alkaline aqueous solution is also returned to the AL container 118 via the lines L14 and L22. Thus, after the cleaning of the fractionation film 1141 is completed, the tobacco extract fractionation operation is restarted by the above-described method.
　以下、本発明を実施例により説明するが、本発明はそれにより限定されるものではない。 Hereinafter, although an example explains the present invention, the present invention is not limited by it.
　実施例１および比較例
　本実施例では、図１に示す装置を用いて分画操作を行った。逆浸透膜としては、ＧＥウォーター・テクノロジーズ製Duratherm Excel RO 4040HRを用いた。 Example 1 and Comparative Example In this example, fractionation operation was performed using the apparatus shown in FIG. As the reverse osmosis membrane, Duratherm Excel RO 4040HR manufactured by GE Water Technologies was used.
　まず、温度６０℃で、タバコ葉スクラップ（黄色種とバーレー種の混合物）と中骨スクラップの混合物からなるタバコスクラップ４５ｋｇを水２２５Ｌと混合し、撹拌することによりタバコ刻みの抽出を行った。得られた抽出混合物をろ過し、タバコ抽出液と、抽出残渣に分けた。タバコ抽出液中のＴＳＮＡ（ＮＮＮ、ＮＮＫ、ＮＡＴおよびＮＡＢの合計）の濃度を、クロマトグラフィーにより測定したところ、４２４ｍｇ／ｍ3であった。 First, at a temperature of 60 ° C., 45 kg of tobacco scrap consisting of a mixture of tobacco leaf scrap (mixture of yellow and Burley seeds) and medium bone scrap was mixed with 225 L of water, and the tobacco was extracted by stirring. The obtained extraction mixture was filtered and divided into tobacco extract and extraction residue. The concentration of TSNA (total of NNN, NNK, NAT and NAB) in the tobacco extract was measured by chromatography and found to be 424 mg / m 3 .
　抽出残渣を抄紙して、再生タバコウエブを得た。他方、タバコ抽出液をＴＥＬ容器１１１に導入した。 The extracted residue was papered to obtain a regenerated tobacco web. On the other hand, the tobacco extract was introduced into the TEL container 111.
　つぎに、マイクロバブル発生装置１１３（ナゴヤ大島社製）によりマイクロバブルを発生させ、そのマイクロバブルを含むタバコ抽出液をＴＥＬ容器１１１に導入し、析出した析出物（浮遊物）を除去した。この析出物を除去したタバコ抽出液を１バッチ量（３３．５Ｌ）ＴＴＥ容器１１２に入れ、上に述べたように、分画膜（逆浸透膜）１１４１による分画操作に連続的に、膜不透過物画分中のＴＳＮＡの量が、初期量の４．５％（除去率９５．５％）となるまで行った。最終的に得られた膜不透過物画分中のニコチンは、初期量の約８６．６％を維持していた。こうして得られた膜不透過物画分を、前記再生タバコウエブに添加して、再構成タバコ材を得た。このようにして、６０バッチ量のタバコ抽出液を処理し、１２バッチ量のタバコ抽出液を処理した後毎に分画膜の洗浄（７８℃の温水による洗浄、マイクロバブルによる洗浄および水酸化ナトリウム水溶液による洗浄各２０分）を行った。 Next, microbubbles were generated by a microbubble generator 113 (Nagoya Oshima Co., Ltd.), a tobacco extract containing the microbubbles was introduced into the TEL container 111, and the deposited precipitates (floating matter) were removed. The tobacco extract from which this precipitate has been removed is put into a batch (33.5 L) TTE vessel 112, and as described above, the membrane is continuously subjected to the fractionation operation by the fractionation membrane (reverse osmosis membrane) 1141. This was performed until the amount of TSNA in the impermeate fraction reached 4.5% of the initial amount (removal rate 95.5%). The nicotine in the final membrane-impermeable fraction was maintained at about 86.6% of the initial amount. The membrane impermeate fraction thus obtained was added to the regenerated tobacco web to obtain a reconstituted tobacco material. In this way, 60 batches of tobacco extract were processed, and each time after 12 batches of tobacco extract were processed, the separation membrane was washed (washing with warm water at 78 ° C., washing with microbubbles and sodium hydroxide). Washing with an aqueous solution for each 20 minutes).
　また、比較例として、マイクロバブルによるタバコ抽出液の前処理を行わなかった以外は上記と同様にして分画操作を行った。 As a comparative example, the fractionation operation was performed in the same manner as above except that the pretreatment of the tobacco extract with microbubbles was not performed.
　それぞれの場合の初期膜透過流束に対する１バッチ量のタバコ抽出液の処理後の膜透過流束の比（膜透過流束比）を図２に示す。膜透過流束は、流量計により測定した。図２において、黒丸印は、マイクロバブルによる前処理を行った場合の結果を、×印は、前処理を行わなかった場合の結果を示す。 FIG. 2 shows the ratio of membrane permeation flux (membrane permeation flux ratio) after treatment of one batch of tobacco extract to the initial membrane permeation flux in each case. The membrane permeation flux was measured with a flow meter. In FIG. 2, black circles indicate the results when pre-processing with microbubbles is performed, and x marks indicate the results when no pre-processing is performed.
　図２からわかるように、マイクロバブルによる前処理を行った場合は、前処理を行わなかった場合に比べ、膜透過流束の低下がほぼ半減している。このことから、タバコ抽出液をマイクロバルブで前処理することにより、逆浸透膜の連続使用時間が有意に延長されることが分かる。 As can be seen from FIG. 2, when the pretreatment with microbubbles is performed, the decrease in the membrane permeation flux is almost halved as compared with the case where the pretreatment is not performed. This shows that the continuous use time of a reverse osmosis membrane is significantly extended by pre-processing a tobacco extract with a microvalve.
　実施例２
　実施例１と同様の分画操作を行い、１２バッチ量のタバコ抽出液を処理した後毎に分画膜の洗浄（７８℃の温水による洗浄および水酸化ナトリウム水溶液による洗浄各２０分）を行った。このようにして、１６７バッチ量のタバコ抽出液の分画と洗浄を行い、次の、１６８バッチ目のタバコ抽出液の分画を行った後、７８℃の温水による洗浄、マイクロバブルによる洗浄および水酸化ナトリウム水溶液による洗浄を各２０分間行った。このとき、マイクロバブル含有洗浄液にオゾン発生器１１６（ナゴヤ大島社製）から発生させたオゾンを供給した。洗浄終了後ついで、１６９～１８０バッチ目のタバコ抽出液の分画操作を行った。１バッチ量のタバコ抽出液の処理後の膜透過流束比を図３に示す。図３からわかるように、通常の温水／アルカリ水溶液による洗浄では除去が困難な膜閉塞物質をマイクロバブル洗浄により効果的に除去することができ、逆浸透膜の連続使用時間が有意に延長されることが分かる。 Example 2
The same fractionation operation as in Example 1 was performed, and after each batch of tobacco extract was treated, the fractionation membrane was washed (washing with warm water at 78 ° C. and washing with aqueous sodium hydroxide solution for 20 minutes each). It was. In this way, the tobacco extract of 167 batches was fractionated and washed, and after the next 168th batch of tobacco extract was fractionated, washing with warm water at 78 ° C., washing with microbubbles and Washing with an aqueous sodium hydroxide solution was performed for 20 minutes each. At this time, ozone generated from an ozone generator 116 (manufactured by Nagoya Oshima Co., Ltd.) was supplied to the cleaning liquid containing microbubbles. After the washing, fractionation operation was performed on the tobacco extracts of the 169th to 180th batches. The membrane permeation flux ratio after treatment of one batch of tobacco extract is shown in FIG. As can be seen from FIG. 3, membrane blocking substances that are difficult to remove by washing with normal warm water / alkaline aqueous solution can be effectively removed by microbubble washing, and the continuous use time of the reverse osmosis membrane is significantly extended. I understand that.

Claims (7)

  1. 　（ａ）天然タバコ材を抽出溶媒で抽出して、所望成分と不所望成分とを含有するタバコ抽出液および抽出残渣を得ること、（ｂ）前記タバコ抽出液を、マイクロバブルと接触させること、（ｃ）前記マイクロバブルとの接触により前記タバコ抽出液中に析出した析出物を除去すること、（ｄ）前記析出物が除去されたタバコ抽出液を限外ろ過膜または逆浸透膜による分画操作に供して、前記所望成分を含有し、かつ前記不所望成分が貧化された第１の画分と、前記所望成分が貧化され、かつ前記不所望成分が富化された第２の画分とを得ること、（ｅ）前記抽出残渣を含む再生タバコウエブを調製すること、および（ｆ）前記第１の画分を前記再生タバコウエブに添加することを包含する再生タバコ材の製造方法。 (A) extracting a natural tobacco material with an extraction solvent to obtain a tobacco extract containing the desired and undesired components and an extraction residue; (b) contacting the tobacco extract with microbubbles; (C) removing precipitates precipitated in the tobacco extract by contact with the microbubbles; (d) fractionating the tobacco extract from which the precipitates have been removed by an ultrafiltration membrane or a reverse osmosis membrane; A first fraction containing the desired component and having the undesired component deteriorated, and a second fraction having the desired component poor and being enriched with the undesired component. A regenerated tobacco material comprising: (e) preparing a regenerated tobacco web containing the extraction residue; and (f) adding the first fraction to the regenerated tobacco web. Method.
  2. 　前記工程（ｄ）の後、前記分画膜をマイクロバブルを含む洗浄液と接触させることを含む前記分画膜の洗浄プロセスを行う請求項１に記載の方法。 The method according to claim 1, wherein after the step (d), the fractionation membrane is subjected to a washing process including contacting the fractionation membrane with a washing liquid containing microbubbles.
  3. 　前記洗浄液にオゾンを導入することをさらに含む請求項２に記載の方法。 The method according to claim 2, further comprising introducing ozone into the cleaning liquid.
  4. 　前記洗浄プロセスは、温水による前記分画膜の洗浄および／またはアルカリ水溶液による前記分画膜の洗浄をさらに含む請求項２または３に記載の方法。 The method according to claim 2 or 3, wherein the cleaning process further includes cleaning the fractionation membrane with warm water and / or washing the fractionation membrane with an alkaline aqueous solution.
  5. 　タバコ抽出液中の所望成分と不所望成分とを分離するための分画装置であって、タバコ抽出液を収容する第１の容器と、マイクロバブル発生装置と、前記発生したマイクロバブルを、該マイクロバブルで前記タバコ抽出液を処理して前記タバコ抽出液から析出物を析出させるために、前記第１の容器に送給する第１の送給デバイスと、前記マイクロバブルで処理されたタバコ抽出液を、前記所望成分を含有し、かつ前記不所望成分が貧化された第１の画分と、前記所望成分が貧化され、かつ前記不所望成分が富化された第２の画分とに分画する限外ろ過膜または逆浸透膜を備える分画デバイスとを備える装置。 A fractionation device for separating a desired component and an undesired component in a tobacco extract, the first container containing a tobacco extract, a microbubble generator, and the generated microbubbles, A first feeding device that feeds the first container to treat the tobacco extract with microbubbles to deposit precipitates from the tobacco extract; and a tobacco extract treated with the microbubbles A first fraction containing the desired component and wherein the undesired component is poor; and a second fraction wherein the desired component is poor and the undesirable component is enriched. And a fractionation device comprising an ultrafiltration membrane or a reverse osmosis membrane.
  6. 　水を収容する第２の容器と、前記第２の容器に収容された水を前記マイクロバブル発生装置に送給し、前記マイクロバブル発生装置により生み出されたマイクロバブル含有水を前記第２の容器に戻す第２の送給デバイスと、前記分画膜を洗浄するために、前記マイクロバブル含有水を前記分画デバイスに送給する第３の送給デバイスをさらに備える請求項５に記載の分画装置。 A second container for containing water, and water contained in the second container is supplied to the microbubble generator, and the microbubble-containing water produced by the microbubble generator is supplied to the second container. 6. The minute feeding device according to claim 5, further comprising: a second feeding device to be returned to the second feeding device; and a third feeding device for feeding the microbubble-containing water to the fractionation device to wash the fractionation membrane. Drawing device.
  7. 　オゾン発生器をさらに含み、前記オゾン発生器で発生されたオゾンを前記マイクロバブル含有水に導入する請求項６に記載の分画装置。 The fractionation device according to claim 6, further comprising an ozone generator, wherein the ozone generated by the ozone generator is introduced into the water containing microbubbles.
PCT/JP2011/058341 2011-03-31 2011-03-31 Process and apparatus for producing regenerated tobacco material WO2012132007A1 (en)

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Cited By (4)

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CN106509975A (en) * 2017-01-16 2017-03-22 云南瑞升烟草技术（集团）有限公司 Method for regulating key chemical component content of reconstituted tobacco
CN110720659A (en) * 2019-10-22 2020-01-24 云南中烟工业有限责任公司 Method for effectively improving quality of reconstituted tobacco

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